Process for the recovery of the unsaponifiable fractions of oils



Patented Dec. 21, 1937 1 PROCESS FOR THE RECOVERY OF THE UN-SAPONIFIABLE FRACTIONS OF OILS Robert Preston Nichols, Miami, Fla.,assignor to Edward L. Nichols, Hollywood, Fla.

No Drawing. Application September 19, 1933, Serial No. 690,107

2 Claims. (Cl. 260-153) My invention relates to a process of recoveringthe contents into the pans as soon as the mass unsaponifiable fractionsof fats, and is particubecomes thick. Ordinarily a cool solidified soaplarly adaptable for use in extracting suchfracmass will be formed in notover twenty minutes tions of cod liver oil, shark liver oil, and thelike. from the time the lye is added to the container.

The invention, which has among its objects a The soap mass formed asabove described conquickly performed process requiring inexpensive tainsmixed with it the unsaponifiable portions apparatus, will be bestunderstood from the folcontaining the vitamins A and D. The soap masslowing description of several examples of the may now be treated toremove these portions. practice of the process, while the scope of thePreferably this is done by first breaking up the m invention will bemore particularly pointed out in soap mass, and then treating it with avolatile the appended claims. organic solvent for the unsaponifiablematter.

As is well known, the unsaponifiable portions As suitable solvents,ether, carbon tetrachlorid, of fats, such as cod liver and shark liveroils, chloroform, or the like, in which the soap and contain thevaluable vitamins A and D. As the alkali are only minutely soluble, maybe em- ]5 improved process lends itself to performance with ployed.Conveniently, the pans employed for a minimum of exposure of thematerials to air, solidifying the soap mass may be in the form of lightand moisture, it is particularly adaptable troughs to cause thesolidified mass to be in the for extracting these vitamins, the latter,particuform of elongated sticks say, for example, sticks larly vitaminA, being susceptible to destruction about one inch square, these beingreadily pre- 90 when the material is so exposed. sented to a grindingmachine which will break As one manner of practising the present invenph S p into a o se Pow ertion, but without limitation thereto, the fattyma- The xtr t n f the n pon fi le p rtions terial, such as cod liveroil, may be placed in a from the P d d broken 1 Seal) mass y container,after .which is added dry powdered be p r rm d y p a th s ap p wd r n asodium hydroxid in the form of co me i l l container and adding theether orother volatile for example, one containing about 98% sodium Svent a d Stirring e nt ts f e Conhydroxid. the lye being addedpreferably as a tainer. Upon being allowed to stand the soap mass asdistinguished from gradually adding it, will settle at the bottom of thecontainer, after Preferably, the amount of lye added is such as Whichthe liquid Contents may be decanted,

to present an amount of sodium hydroxid in expri r t s ttl n the s apmay be s pa ated fr m 30 cess of that necessary to saponify thesaponifiable the qu d by us f a tr u al s parat r r y fats in the oil,so as to cause the moisture to be use Of a filter- It has b found thatug y 10 absorbed and the vitamins to be thus protected p s v nt to one prt ap will i i fa from this moisture. In practice, equal portions Yresults, but these P op are y I10 by weight of the oil and sodiumhydroxid in the fii C t calform of commercial lye give satisfactoryresults. The ether or other solution of the unsaponi- Immediately uponintroducing the lye the confiable fractions, separated as abovedescribed,

tents of the container are intimately mixed as, for may be then treatedby a distilling operation to example, by use of a mechanical mixer.Pracremove the solvent, distillation preferably being ticallyimmediately, saponification begins, the performed under reduced pressureand at a 40 temperature of the contents of the container rlstemperaturenot exceeding 100 C. By this means ing rapidly and saponificationproceeding at a a concentrate rich in the vitamins A and D is rapidrate, so that in a few minutes the mass recovered. Any small fraction ofsoap present becomes thick and pasty. At this point the main theconcentrate may be removed, if desired,

terial is preferably poured into pans to permit the by treating theconcentrate with a small amount 45 saponification reaction to becomecomplete and of ether, or other of the above mentioned solthe materialto cool and harden into a block of vents in which the soap is only veryslightly solusoap, If desired, the oil may be slightly heated ble, todissolve off the unsaponifiable matter and before adding the lye toinitiate the saponificaleave the soap behind, or the concentrate, whichtion reaction, but ordinarily this will be unordinarily is in the formof a rather thick paste, 50 necessary. Preferably, care should be takennot may be diluted with cod liver oil, corn oil, cotton to give such aninitial heating as will cause the seed oil, peanut oil, or the like, inwhich the soap temperature of the mass, when the reaction 00- is notsoluble, and the solution filtered or subcurs, to rise above from to C.This ex- ,iected to centrifugal action to remove the soap.

55 cess temperature may be prevented by pouring Commonly the concentrateis used to enrich the 55 vitamin content of cod liver or other oils, andmay be added thereto, and any soap present may be removed by filteringor centrifugal action.

In the above examples of the practice of the invention, any residualamount of ether or other solvent present in the separated soap may berecovered for reuse, preferably by a distilling operation.

It will be observed in the above examples of the practice of my improvedprocess, that the excess of lye or other hydroxid added to the oil notonly saponifies the fatty fractions, but being in amount in excess ofthat necessary to form the soap, also takes up the moisture so that theunsaponifiable fractions are not subjected to moisture during theprocess. This materially aids in the recovery of a high percentage ofthe vitamin A which tends to be destroyed, at least in part, whensubjected to moisture, particularly in the presence of heat.

It will be understood that wide deviations may be made from the aboveexamples of the practice of my invention without departing from thespirit thereof.

I claim:

1. The process of recovering the unsaponifiable fractions of fish liveroil which comprises adding to and immediately mixing with the oil drypowdered sodium hydroxide, the latter being added to the oilsubstantially as a mass in large excess over that necessary to saponifythe saponifiable fractions of the oil, so as to absorb moisture forprotecting the vitamins and cause to be quickly formed a solidifiedmixture of soap and sodium hydroxide of requisite hardness to be reducedto a powder by a grinding operation; operating upon said solidifiedmixture to grind it to a powder; treating the resulting powder withether for dissolving the unsaponified fractions of the oil; separatingthe powder from the ether solution; and distilling the ether from thepowder free ether solution to obtain a concentration of theunsaponifiable fractions of the oil.

2. The process of recovering the unsaponifiable fractions of fish liveroil which comprises adding to and immediately mixing with the oil drypowdered sodium hydroxide, the latter being added to the oilsubstantially as a mass in large excess over that necessary to saponifythe saponifiable fractions of the oil, so as to absorb moisture forprotecting the vitamins and cause to be quickly formed a solidifiedmixture of soap and sodium hydroxide of requisite hardness to be reducedto a powder by a grinding operation; operating upon said solidifiedmixture to grind it to a powder; treating the resulting powder with avolatile liquid in which both the unsaponifiable and saponifiablefractions of the oil are soluble, but in which both the soap and sodiumhydroxide are insoluble, for dissolving the unsaponified fractions ofthe oil from the powder; separating the powder from the resultingsolution of the unsaponified fractions of the oil; and treating thepowder free solution for vaporizing the volatile liquid solventtherefrom to obtain a concentration of the unsaponifiable fractions ofthe oil.

ROBERT PRESTON NICHOLS.

